JP4381760B2 - Flexible ceramic product and manufacturing method thereof - Google Patents
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Description
本発明は、可撓性セラミックス製品及びその製造方法に関する。 The present invention relates to a flexible ceramic product and a manufacturing method thereof.
セラミックスの分野において、部分安定化ジルコニアという物が発明され、高強度・高靱性のセラミックス製のナイフやはさみが製造されるようになった。これは多少撓むことができ、外からの応力は結晶変態の転移によって緩和される。以来、他のセラミックスに対しても粒径のコントロールや複合化によって高強度・高靱性のセラミックスが開発されている（例えば、特許文献１）。その応力緩和機構の一つとしてマイクロクラックの存在がある。 In the field of ceramics, a partially stabilized zirconia was invented, and high-strength and high-toughness ceramic knives and scissors have come to be manufactured. This can be somewhat deflected, and the external stress is relaxed by the transition of the crystal transformation. Since then, ceramics having high strength and high toughness have been developed by controlling the particle size and combining them with other ceramics (for example, Patent Document 1). One of the stress relaxation mechanisms is the presence of microcracks.
一般のセラミックスは応力が加わったとき、ほとんど変位しないまま破壊するのに対
し、マイクロクラックを持ったセラミックスでは変位量が多少増え、これは靱性が向上したとかヤング率が低下したという事実として説明される。しかし、マイクロクラックによる変位量（撓む程度）は、目に見えるほどではない。
In general, ceramics break with little displacement when stress is applied, whereas in ceramics with microcracks, the amount of displacement increases somewhat, which is explained as the fact that the toughness is improved and the Young's modulus is reduced. The However, the amount of displacement (the degree of bending) due to microcracks is not appreciable.
セラミックスは小さな結晶粒子の集合体であり、それらはいろいろな方向を向いている。そして、Ｘ、Ｙ、Ｚ軸方向の熱膨張係数が大きく異なる場合、違う方向の結晶面が隣り合った時、冷却過程で縮む程度が異なるため、結晶粒界に応力が発生してクラックが生成する。マイクロクラックの発生は結晶粒子の大きさと軸方向の熱膨張係数の差によって決まる。 Ceramics are aggregates of small crystal particles that are oriented in various directions. And if the thermal expansion coefficients in the X, Y, and Z axis directions are greatly different, when crystal planes in different directions are adjacent to each other, the degree of shrinkage in the cooling process is different, so stress is generated at the crystal grain boundaries and cracks are generated. To do. The occurrence of microcracks is determined by the difference between the size of crystal grains and the coefficient of thermal expansion in the axial direction.
一般にセラミックスの粒径はサブミクロンからせいぜい数十ミクロンの範囲であり、結晶軸方向の熱膨張係数の差が5×10-6／℃以上になると、マイクロクラックが発生する場
合が多くなる。そして、クラックもその名が示すようにマイクロメーターの大きさである。本発明者らは、熱膨張係数の差によりセラミックス中の結晶粒界にマイクロクラックが発生する条件について、既に報告している（非特許文献１）。
In general, the grain size of ceramics is in the range of submicron to tens of microns at most, and microcracks often occur when the difference in thermal expansion coefficient in the crystal axis direction is 5 × 10 −6 / ° C. or more. And as the name suggests, cracks are the size of a micrometer. The present inventors have already reported the conditions under which microcracks are generated at the grain boundaries in ceramics due to the difference in thermal expansion coefficient (Non-Patent Document 1).
一方、天然で可撓性を有する材料（鉱物）としてはコンニャク石という通称で知られるイタコルマイトが知られているが、産地は世界に数カ所であり、産出量も非常に僅かである。コンニャク石の場合は粒径及びクラックの大きさは数十μｍから数百μｍのオーダーで、曲がるのが目視できるほどになる。人工的に、コンニャク石と類似の可撓性を付与したセラミックスとしては、粒界部分を溶解することによって隙間を作る例が知られている（例えば、特許文献２）程度である。 On the other hand, itacorumite, commonly known as konjac stone, is known as a natural and flexible material (mineral), but it is produced in several places in the world and its output is very small. In the case of konjak stone, the particle size and the crack size are on the order of several tens of μm to several hundreds of μm, and the bending is visible. Artificially, an example of creating a gap by dissolving a grain boundary part is known as a ceramic having flexibility similar to konjac stone (for example, Patent Document 2).
セラミックスは共有結合やイオン結合の結晶体であるために高強度であるが、靭性が乏しく、塑性変形しない、曲がらないなど、可撓性に劣っている。セラミックスにコンニャク石と同等以上の十分な可撓性を付与できれば、従来制約されていた用途へのセラミックスの利用を促進できる。 Ceramics are high in strength because they are covalently bonded or ionic bonded crystals, but they are poor in flexibility, such as poor toughness, plastic deformation and bending. If sufficient flexibility equivalent to or higher than that of konjac stones can be imparted to ceramics, it is possible to promote the use of ceramics for applications that have been conventionally restricted.
本発明は、熱膨張係数と粒径の異なるセラミックス粒子を混合、成形、焼成して、粒界にクラックによって３次元的に空隙を発生させ、クラックを応力緩和機構として挙動させることによって上記の課題を解決したものである。 The present invention solves the above problem by mixing, forming and firing ceramic particles having different thermal expansion coefficients and particle sizes, generating voids three-dimensionally by cracks at the grain boundaries, and causing the cracks to behave as a stress relaxation mechanism. Is a solution.
すなわち、本発明は、（１）複合する一方の成分は熱膨張係数が2×10-6／℃以下の低
熱膨張性セラミックスであり、もう一方の成分はそれよりも5×10-6／℃以上大きい熱膨
張係数を有する高熱膨張性セラミックスであり、かつどちらか一方の成分は平均粒径100
μｍ〜500μｍの粒子であり、他方の成分は平均粒径10μｍ以下であるセラミックス粒子
を混合し、成形・焼成したセラミックスであって、粒界に粒子同士の熱膨張係数の差によって発生した３次元的に連続した開放気孔としてのクラックを5〜20容積％持つことを特
徴とする可撓性セラミックス製品、である。
また、本発明は、（２）高熱膨張性セラミックスは、熱膨張係数が20×10-6／℃以上のものであることを特徴とする上記（１）の可撓性セラミックス製品、である。
That is, in the present invention, (1) one component to be combined is a low thermal expansion ceramic having a thermal expansion coefficient of 2 × 10 −6 / ° C. or less, and the other component is 5 × 10 −6 / ° C. It is a high thermal expansion ceramic having a large thermal expansion coefficient, and either component has an average particle size of 100.
Three-dimensional particles generated by mixing the ceramic particles with an average particle size of 10 μm or less, and molding and firing them, due to the difference in thermal expansion coefficient between the particles. A flexible ceramic product characterized by having 5 to 20% by volume of cracks as continuous open pores.
The present invention also provides the flexible ceramic product according to (1), wherein (2) the high thermal expansion ceramic has a thermal expansion coefficient of 20 × 10 −6 / ° C. or more.
また、本発明は、（３）平均粒径100μｍ〜500μｍの粒子は100μｍより小さい単一相
の小さい粒子を予め焼結させたものであることを特徴とする上記（１）又は（２）の可撓性セラミックス製品、である。
In the present invention, (3) the particles having an average particle diameter of 100 μm to 500 μm are obtained by previously sintering small particles having a single phase smaller than 100 μm. Flexible ceramic products.
また、本発明は、（４）該開放気孔としてのクラックに樹脂及び／又は金属を持つことを特徴とする上記（１）ないし（３）のいずれかの可撓性セラミックス製品、である。 The present invention is also (4) the flexible ceramic product according to any one of (1) to (3) above, wherein the cracks as the open pores have a resin and / or a metal.
また、本発明は、（５）熱膨張係数及び粒径の異なるセラミックス粒子を２種以上混合し、成形、焼成して、粒界に粒子同士の熱膨張係数の差によって３次元的に連続した開放気孔としてのクラックを発生させることを特徴とする上記（１）ないし（３）のいずれかの可撓性セラミックス製品の製造方法、である。 In the present invention, (5) two or more kinds of ceramic particles having different thermal expansion coefficients and particle sizes are mixed, molded and fired, and three-dimensionally continuous at the grain boundaries due to the difference in thermal expansion coefficients between the particles. A method for producing a flexible ceramic product according to any one of (1) to (3), wherein cracks as open pores are generated.
また、本発明は、（６）上記（５）の方法で発生させた３次元的に連続した開放気孔としてのクラックに樹脂及び／又は金属を含浸させることを特徴とする上記（４）の可撓性セラミックス製品の製造方法、である。 Further, the present invention provides (6) the above (4), wherein a crack as a three-dimensional continuous open pore generated by the method of (5) is impregnated with resin and / or metal. A method for manufacturing a flexible ceramic product.
イタコルマイトは石英型SiO2であり、その空隙率が5〜20容積％であり、粒子はジクソ
ーパズルの様に噛み合って３次元の粒界隙間を有しているため、応力緩和機構として働き、変形可能であるが、本発明は、通常のセラミックスの製造工程を用いて、人工的にコンニャク石と同等以上の十分な可撓性を有し、塑性変形するセラミックスを提供することができた。
Itacormite is a quartz-type SiO 2 with a porosity of 5-20% by volume, and the particles mesh like a jigsaw puzzle and have a three-dimensional grain boundary gap. However, the present invention was able to provide a ceramic that has a sufficient flexibility equivalent to or higher than that of konjak and can be plastically deformed by using a normal ceramic manufacturing process.
図１は、本発明の原理を概念的に示す説明図である。原料粉末としては、熱膨張係数の異なるセラミックス粒子を２種以上混合する。複合する一方の成分は熱膨張係数が2×10-6／℃以下の低熱膨張性セラミックスであり、もう一方の成分はそれよりも5×10-6／℃以上大きい熱膨張係数を有する高熱膨張性セラミックスであり、かつどちらか一方の成分は平均粒径100μｍ〜500μｍの粒子であり、他方の成分は平均粒径10μｍ以下であるセラミックス粒子を混合する。 FIG. 1 is an explanatory diagram conceptually showing the principle of the present invention. As the raw material powder, two or more kinds of ceramic particles having different thermal expansion coefficients are mixed. One component is a low thermal expansion ceramic with a coefficient of thermal expansion of 2 × 10 -6 / ° C or less, and the other component is a high thermal expansion with a coefficient of thermal expansion that is 5 × 10 -6 / ° C or higher. Ceramic particles, and either component is particles having an average particle size of 100 μm to 500 μm, and the other component is mixed with ceramic particles having an average particle size of 10 μm or less.
すなわち、複合する組み合わせは、（１）低熱膨張係数の平均粒径が100μｍ〜500μｍ程度の粒子とその粒界相としての高熱膨張係数の平均粒径が10μｍ以下程度もの、又は、（２）高熱膨張係数の100μｍ〜500μｍ程度の粒子とその粒界相としての低熱膨張係数の平均粒径が10μｍ以下程度ものである。なお、平均粒径は数平均粒径である。平均粒径が小さい方の粒子の下限は特に制約はないが、0.1μｍ程度でも特に支障はない。それぞれ
の平均粒子径が前記の範囲を外れるとクラックを十分に発生し難くなる。
That is, the composite combination includes (1) particles having an average particle size of low thermal expansion coefficient of about 100 μm to 500 μm and an average particle size of high thermal expansion coefficient as a grain boundary phase of about 10 μm or less, or (2) high heat The particles having an expansion coefficient of about 100 μm to 500 μm and the average particle diameter of the low thermal expansion coefficient as the grain boundary phase are about 10 μm or less. The average particle size is the number average particle size. The lower limit of the particles having a smaller average particle diameter is not particularly limited, but there is no particular problem even if it is about 0.1 μm. When the average particle diameter is out of the above range, cracks are hardly generated.
平均粒径の大きい粒子が充填された隙間に平均粒径の小さい粒子が詰まる。普通、粒子を充填するとその体積分率は50〜60容積％程度となり、残りの50〜40容積％程度が隙間になる。その隙間の部分を平均粒径の小さい粒子が埋めることになるので、平均粒径の大きい粒子に対して平均粒径の小さい粒子の割合は約50容積％以上でないと、全体が密にならないでクラックでない穴が残ってしまう。 Particles having a small average particle size are clogged in the gap filled with particles having a large average particle size. Usually, when the particles are filled, the volume fraction is about 50 to 60% by volume, and the remaining 50 to 40% by volume becomes a gap. Since the particles with a small average particle diameter are filled in the gaps, the ratio of the particles with a small average particle diameter to the particles with a large average particle diameter is not more than about 50% by volume. Holes that are not cracked remain.
なお、クラックの発生は、平均粒径と熱膨張係数の差が関係し、平均粒径が大きくなるほど熱膨張係数の差は小さくてもクラックが発生する。両者の熱膨張係数の差が5〜10×10-6／℃あれば、平均粒径の大きい方がおおよそ100μｍ〜500μｍの平均粒径で、平均粒
径の小さい方がおおよそ10μｍ以下であれば、クラックは発生し、粒径の大きい方が100
μｍ以上の粒径の場合、成分の一つとして低熱膨張セラミックスを用いれば、もう一方の成分にはジルコニア、アルミナなどの一般のセラミックスを用いてもクラックが発生する。
The occurrence of cracks is related to the difference between the average particle diameter and the thermal expansion coefficient. The larger the average particle diameter, the more the cracks are generated even if the difference in thermal expansion coefficient is small. If the difference in thermal expansion coefficient between the two is 5 to 10 × 10 −6 / ° C., the larger average particle size is about 100 μm to 500 μm and the smaller average particle size is about 10 μm or less. , Cracks occur, the larger the particle size is 100
In the case of a particle size of μm or more, if a low thermal expansion ceramic is used as one of the components, cracks are generated even if a general ceramic such as zirconia or alumina is used for the other component.
複合する一方の成分として熱膨張係数が2×10-6／℃以下の低熱膨張性セラミックスを
用い、もう一方の成分として熱膨張係数が20×10-6／℃以上の高熱膨張性セラミックスを用いると粒界にクラックを発生させることが容易になるのでより好ましい。
Use low thermal expansion ceramics with a thermal expansion coefficient of 2 × 10 −6 / ° C. or lower as one component and use high thermal expansion ceramics with a thermal expansion coefficient of 20 × 10 −6 / ° C. or higher as the other component. It is more preferable because it is easy to generate cracks at the grain boundaries.
例えば、KZr2(PO4)3リン酸ジルコニウムカリウム(KZP)は低熱膨張係数(−0.4×10-6／
℃)の物質である。また、KAlSi2O6リューサイト(L)は高熱膨張係数(25×10-6／℃の物質
である。KZPとして粒径の大きいものを用い、リューサイト(L)として粒径の小さいものを用い、大きなKZP粒子：小さなL粒子＝30：70〜20：80程度とした場合、焼成後、冷却すると粒径の大きなKZP粒子の周りのリューサイト(L)が収縮するのでクラックが発生する。これと逆の場合は、粒径の大きなリューサイト(L)が収縮するためクラックが生じると考え
られる。このクラックが空隙として働く。
For example, KZr 2 (PO 4 ) 3 potassium potassium phosphate (KZP) has a low coefficient of thermal expansion (−0.4 × 10 −6 /
℃) substance. KAlSi 2 O 6 leucite (L) is a material with a high coefficient of thermal expansion (25 × 10 -6 / ° C. A material with a large particle size is used as KZP and a material with a small particle size is used as leucite (L). When using large KZP particles: small L particles = 30: 70 to 20:80, cracking occurs because the leucite (L) around the large KZP particles shrinks when cooled after firing. In the opposite case, it is considered that cracks are generated because leucite (L) having a large particle size contracts, and these cracks act as voids.
本発明のセラミックス製品の製造工程自体は、通常のセラミックス製品の製造工程と異ならず、原料粉末に適宜焼結促進剤を混合して、所要の形状にプレス成形し、所要の温度で焼成する。本発明は、原料粉末の選択と、該原料粉末に応じた焼成温度で焼成することに特徴を有する。 The manufacturing process itself of the ceramic product of the present invention is not different from the manufacturing process of a normal ceramic product, and a raw material powder is appropriately mixed with a sintering accelerator, press-formed into a required shape, and fired at a required temperature. The present invention is characterized by selection of raw material powder and firing at a firing temperature according to the raw material powder.
複合する粉末としては２種類の成分が焼成過程において反応しないものを選択することが好ましい。平均粒径100μｍ〜500μｍの粒子は平均粒子が100μｍよりも小さい単一相
の粒子を焼結させて大きな二次粒子を作っておいてから、別の成分である小さい粒子と混合し、次に、小さい粒子だけが焼結して全体を固めるようにすることによって、焼成過程における２種類の成分の反応を防ぐことができる。焼成温度条件は原料粉末及び添加剤の種類と量によって実験的に最適条件を選択する。
As the powder to be combined, it is preferable to select a powder in which two kinds of components do not react in the firing process. Particles with an average particle size of 100 μm to 500 μm are sintered with single-phase particles whose average particle is smaller than 100 μm to make large secondary particles, and then mixed with small particles as other components, By making only small particles sinter and harden the whole, the reaction of the two types of components in the firing process can be prevented. The optimum firing temperature condition is selected experimentally depending on the kind and amount of the raw material powder and additive.
このような原料の組み合わせを用いて焼成した後冷却すると、焼結体の粒界に３次元的なクラックが発生する。マイクロクラックの発生に関しては、２つの成分の界面において、（その熱膨張係数の差）×（粒径）×（焼成温度と冷却後の温度(通常は室温）との最
終的な温度差）で応力が決まるので、冷却速度はあまり関係がない。通常のセラミックスにおいて冷却速度が速い場合、セラミックス製品の表面と内部の温度差によってクラックが発生することがあるが、その場合は破壊に至る大きな割れとなる。
When fired using such a combination of raw materials and then cooled, three-dimensional cracks are generated at the grain boundaries of the sintered body. Regarding the occurrence of microcracks, at the interface between two components, (difference in thermal expansion coefficient) x (particle size) x (final temperature difference between firing temperature and temperature after cooling (usually room temperature)) Since the stress is determined, the cooling rate is not very relevant. When the cooling rate is high in normal ceramics, cracks may occur due to the temperature difference between the surface and the inside of the ceramic product. In this case, the cracks are large leading to breakage.
空隙率に関してはコンニャク石と同程度の5〜20容積％程度が好ましい。一般のセラミ
ックスにおいて、空隙率が5容積％未満になると主に閉気孔になるので、それ以上が必要
である。また20容積％程度を超えると、クラック以外の大きな気孔（穴）の存在が顕著と
なり、粒子同士の絡み合いが困難となる。なお、空隙率は試料の重量と見かけの体積等を用いてアルキメデス法によって測定した開気孔率である。
The porosity is preferably about 5 to 20% by volume, which is the same as konjac stone. In general ceramics, when the porosity is less than 5% by volume, closed pores are mainly formed. On the other hand, if it exceeds about 20% by volume, the presence of large pores (holes) other than cracks becomes remarkable, and it becomes difficult to entangle particles. The porosity is an open porosity measured by the Archimedes method using the weight of the sample and the apparent volume.
このクラックは連続開放空隙であるので、一般に用いられている多孔体へのポリマー及び金属の含浸法によりエポキシ樹脂やシリコーンゴムなどのポリマー及び／又はアルミニウムや珪素などの金属を含浸させてもよい。 Since this crack is a continuous open space, a polymer such as an epoxy resin or silicone rubber and / or a metal such as aluminum or silicon may be impregnated by a generally used method of impregnating a porous body with a polymer and metal.
実施例１
低熱膨張係数(−0.4×10-6／℃)で粒径が2μｍ以下のリン酸ジルコニウムカリウム(KZP)粉体を100重量部を取り、焼結促進剤として酸化マグネシウムを2重量部加えて十分混合
しペレット状に成形た後、1300℃で焼成した。冷却後これを粉砕し、ふるいにより平均粒径が100μｍ〜250μｍのKZP粒子を作成した。
Example 1
Take 100 parts by weight of potassium zirconium phosphate (KZP) powder with a low coefficient of thermal expansion (-0.4 × 10 -6 / ° C) and a particle size of 2 μm or less, and add 2 parts by weight of magnesium oxide as a sintering accelerator. After mixing and forming into a pellet, it was fired at 1300 ° C. After cooling, this was pulverized and KZP particles having an average particle diameter of 100 μm to 250 μm were prepared by sieving.
次に、高熱膨張係数(25×10-6／℃)で粒径が2μｍ以下のリューサイト(L)粉体80重量部と、上記のKZP粒子20重量部並びに、焼結促進剤として炭酸リチウムを5重量部加えて十分混合した後、金型に充填し、一軸プレス成形機を用いて100MPaで5分間一軸加圧成形した
。その試料をセラミック焼成用の電気炉において1200℃、4時間酸化雰囲気中で焼成した
。
Next, 80 parts by weight of leucite (L) powder having a high thermal expansion coefficient (25 × 10 −6 / ° C.) and a particle size of 2 μm or less, 20 parts by weight of the above KZP particles, and lithium carbonate as a sintering accelerator After adding 5 parts by weight, the mixture was sufficiently mixed, filled in a mold, and uniaxially press-molded at 100 MPa for 5 minutes using a uniaxial press molding machine. The sample was fired in an oxidizing atmosphere at 1200 ° C. for 4 hours in an electric furnace for ceramic firing.
得られた焼結体の粒界を電子顕微鏡で観察した結果を図２の左上写真及び右上写真（左上写真の10倍の倍率）に示す。また、比較のために、イタコルマイトの電子顕微鏡像を左下写真及び右下写真（左下写真の10倍の倍率）に示す。図２に示されるとおりに、実施例で得られた焼結体の粒界には、天然のイタコルマイトと類似のクラックが３次元的に生じているのが観察された。 The results of observing the grain boundaries of the obtained sintered body with an electron microscope are shown in the upper left photograph and upper right photograph (magnification of 10 times the upper left photograph) in FIG. For comparison, an electron microscope image of itacolumite is shown in the lower left photograph and lower right photograph (magnification of 10 times that of the lower left photograph). As shown in FIG. 2, it was observed that cracks similar to natural itacolumite were generated three-dimensionally at the grain boundaries of the sintered bodies obtained in the examples.
また、図３に、３点曲げ試験による応力−歪み曲線を示す。図３の（１）及び（２）は、それぞれ、KZPとリューサイトの単一成分焼結体、（３）は、イタコルマイト、（４）
は、本実施例で得られた焼結体である。図３に示すように、単一成分焼結体のKZPやリュ
ーサイトセラミックスの場合と異なり、本実施例で得られた焼結体では天然のイタコルマイトと類似の曲線を示すことが分かった。さらに、得られた焼結体の重量と見かけの体積等を用いてアルキメデス法によって測定した空隙率は約10容積％であった。
FIG. 3 shows a stress-strain curve by a three-point bending test. (1) and (2) in FIG. 3 are respectively a single component sintered body of KZP and leucite, (3) is itacolumite, (4)
Is a sintered body obtained in this example. As shown in FIG. 3, it was found that the sintered body obtained in this example showed a curve similar to that of natural itacolumite, unlike the case of single component sintered body KZP or leucite ceramics. Furthermore, the porosity measured by the Archimedes method using the weight and apparent volume of the obtained sintered body was about 10% by volume.
本発明のセラミックス製品は、塑性変形により撓むので、弾力のある、歩行感の良い床材、地震などの揺れを減少させる防振材、衝撃吸収材、弾力性のある壁材・屋根材などへの用途が考えられる。 Since the ceramic product of the present invention bends due to plastic deformation, the floor material is elastic and has a good feeling of walking, vibration-proof material that reduces vibration such as earthquake, shock absorbing material, elastic wall material and roof material, etc. Possible uses for
Claims (6)
もう一方の成分はそれよりも5×10-6／℃以上大きい熱膨張係数を有する高熱膨張性セラ
ミックスであり、かつどちらか一方の成分は平均粒径100μｍ〜500μｍの粒子であり、他方の成分は平均粒径10μｍ以下であるセラミックス粒子を混合し、成形・焼成したセラミックスであって、粒界に粒子同士の熱膨張係数の差によって発生した３次元的に連続した開放気孔としてのクラックを5〜20容積％持つことを特徴とする可撓性セラミックス製品
。 One component of the composite is a low thermal expansion ceramic having a thermal expansion coefficient of 2 × 10 −6 / ° C. or less,
The other component is a high thermal expansion ceramic having a thermal expansion coefficient larger than that by 5 × 10 −6 / ° C., and either component is a particle having an average particle size of 100 μm to 500 μm, and the other component Is a ceramic that has been mixed and molded with ceramic particles with an average particle size of 10 μm or less, and cracks as three-dimensional continuous open pores generated by the difference in thermal expansion coefficient between the particles at the grain boundary. Flexible ceramic product characterized by having ~ 20% by volume.
せたものであることを特徴とする請求項１又は２記載の可撓性セラミックス製品。 The flexible ceramic product according to claim 1 or 2, wherein the particles having an average particle size of 100 µm to 500 µm are obtained by previously sintering small particles having a single phase smaller than 100 µm.
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